#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318237.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4318237
loop_
_publ_author_name
'Sherrika Daniel'
'David M. Hoffman'
_publ_section_title
;
 Synthesis and Structures of Aluminum Alkanethiolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3843
_journal_page_last               3849
_journal_paper_doi               10.1021/ic011257g
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C24 H54 Al2 S6'
_chemical_formula_weight         588.99
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.565(2)
_cell_angle_beta                 62.227(1)
_cell_angle_gamma                74.623(1)
_cell_formula_units_Z            1
_cell_length_a                   9.8289(9)
_cell_length_b                   9.9282(9)
_cell_length_c                   10.1097(9)
_cell_measurement_reflns_used    3236
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.13
_cell_volume                     841.57(13)
_computing_cell_refinement       'Siemens SAINT software (Siemens, 1996)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Siemens SAINT software (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3747
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.8215
_exptl_absorpt_correction_T_min  0.6189
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2349
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0107P)²+3.4463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                2174
_reflns_number_total             2357
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic011257g_1.cif
_cod_data_source_block           k520
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C24 H54 S6 Al2'
_cod_database_code               4318237
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.49895(13) 0.61818(12) 0.37107(12) 0.0211(3) Uani 1 1 d . . .
S2 S 0.89671(14) 0.43159(13) 0.32438(15) 0.0320(4) Uani 1 1 d . . .
S3 S 0.63491(15) 0.23890(13) 0.25913(14) 0.0302(4) Uani 1 1 d . . .
Al Al 0.66435(16) 0.39876(14) 0.37253(15) 0.0208(4) Uani 1 1 d . . .
C1 C 0.5854(5) 0.7759(5) 0.3027(5) 0.0242(10) Uani 1 1 d . . .
C2 C 0.6863(7) 0.7542(6) 0.1355(6) 0.0394(13) Uani 1 1 d . . .
H2A H 0.6214 0.7433 0.0906 0.059 Uiso 1 1 calc R . .
H2B H 0.7717 0.6710 0.1159 0.059 Uiso 1 1 calc R . .
H2C H 0.7304 0.8345 0.0930 0.059 Uiso 1 1 calc R . .
C3 C 0.4426(6) 0.9009(5) 0.3398(7) 0.0383(13) Uani 1 1 d . . .
H3A H 0.3815 0.8884 0.2915 0.057 Uiso 1 1 calc R . .
H3B H 0.4792 0.9858 0.3042 0.057 Uiso 1 1 calc R . .
H3C H 0.3766 0.9078 0.4472 0.057 Uiso 1 1 calc R . .
C4 C 0.6827(6) 0.7935(6) 0.3778(6) 0.0337(12) Uani 1 1 d . . .
H4A H 0.6153 0.8071 0.4845 0.050 Uiso 1 1 calc R . .
H4B H 0.7267 0.8742 0.3369 0.050 Uiso 1 1 calc R . .
H4C H 0.7682 0.7106 0.3597 0.050 Uiso 1 1 calc R . .
C5 C 1.0159(6) 0.2750(5) 0.3752(6) 0.0292(11) Uani 1 1 d . . .
C6 C 0.9495(7) 0.2674(7) 0.5430(7) 0.0484(15) Uani 1 1 d . . .
H6A H 0.9465 0.3538 0.5817 0.073 Uiso 1 1 calc R . .
H6B H 1.0163 0.1898 0.5691 0.073 Uiso 1 1 calc R . .
H6C H 0.8431 0.2536 0.5861 0.073 Uiso 1 1 calc R . .
C7 C 1.1823(6) 0.3002(7) 0.3065(7) 0.0465(15) Uani 1 1 d . . .
H7A H 1.2245 0.3049 0.1986 0.070 Uiso 1 1 calc R . .
H7B H 1.2508 0.2242 0.3323 0.070 Uiso 1 1 calc R . .
H7C H 1.1773 0.3876 0.3450 0.070 Uiso 1 1 calc R . .
C8 C 1.0219(8) 0.1418(6) 0.3099(8) 0.0553(18) Uani 1 1 d . . .
H8A H 1.0647 0.1496 0.2021 0.083 Uiso 1 1 calc R . .
H8B H 0.9157 0.1276 0.3515 0.083 Uiso 1 1 calc R . .
H8C H 1.0890 0.0631 0.3342 0.083 Uiso 1 1 calc R . .
C9 C 0.7486(16) 0.2457(12) 0.054(3) 0.027(4) Uani 0.50 1 d PD A 1
C10 C 0.645(2) 0.2155(19) -0.009(2) 0.051(4) Uani 0.50 1 d PD A 1
H10A H 0.6156 0.1284 0.0310 0.076 Uiso 0.50 1 calc PR A 1
H10B H 0.7038 0.2081 -0.1171 0.076 Uiso 0.50 1 calc PR A 1
H10C H 0.5503 0.2909 0.0191 0.076 Uiso 0.50 1 calc PR A 1
C11 C 0.9036(13) 0.1337(13) -0.0008(14) 0.053(3) Uani 0.50 1 d PD A 1
H11A H 0.8812 0.0424 0.0273 0.079 Uiso 0.50 1 calc PR A 1
H11B H 0.9666 0.1496 0.0439 0.079 Uiso 0.50 1 calc PR A 1
H11C H 0.9619 0.1378 -0.1088 0.079 Uiso 0.50 1 calc PR A 1
C12 C 0.7787(18) 0.3903(13) 0.0049(13) 0.047(3) Uani 0.50 1 d PD A 1
H12A H 0.8340 0.4144 0.0537 0.071 Uiso 0.50 1 calc PR A 1
H12B H 0.6784 0.4584 0.0324 0.071 Uiso 0.50 1 calc PR A 1
H12C H 0.8430 0.3900 -0.1027 0.071 Uiso 0.50 1 calc PR A 1
C9' C 0.7143(17) 0.2798(14) 0.054(3) 0.025(4) Uani 0.50 1 d PD A 2
C10' C 0.709(3) 0.1521(15) -0.014(2) 0.056(5) Uani 0.50 1 d PD A 2
H10D H 0.6054 0.1327 0.0430 0.084 Uiso 0.50 1 calc PR A 2
H10E H 0.7893 0.0720 -0.0102 0.084 Uiso 0.50 1 calc PR A 2
H10F H 0.7296 0.1705 -0.1168 0.084 Uiso 0.50 1 calc PR A 2
C11' C 0.6001(17) 0.4081(13) 0.0320(14) 0.057(4) Uani 0.50 1 d PD A 2
H11D H 0.4954 0.3905 0.0736 0.085 Uiso 0.50 1 calc PR A 2
H11E H 0.6374 0.4269 -0.0739 0.085 Uiso 0.50 1 calc PR A 2
H11F H 0.5950 0.4882 0.0825 0.085 Uiso 0.50 1 calc PR A 2
C12' C 0.8803(16) 0.304(2) -0.0137(16) 0.064(4) Uani 0.50 1 d PD A 2
H12D H 0.8805 0.3766 0.0426 0.096 Uiso 0.50 1 calc PR A 2
H12E H 0.9124 0.3321 -0.1169 0.096 Uiso 0.50 1 calc PR A 2
H12F H 0.9538 0.2181 -0.0099 0.096 Uiso 0.50 1 calc PR A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 Al 118.52(16) . 2_666 ?
C1 S1 Al 119.75(15) . . ?
Al S1 Al 90.32(6) 2_666 . ?
C5 S2 Al 110.81(16) . . ?
C9 S3 C9' 12.6(6) . . ?
C9 S3 Al 111.8(4) . . ?
C9' S3 Al 108.6(4) . . ?
S3 Al S2 123.82(8) . . ?
S3 Al S1 106.66(7) . 2_666 ?
S2 Al S1 112.68(7) . 2_666 ?
S3 Al S1 110.99(7) . . ?
S2 Al S1 107.75(7) . . ?
S1 Al S1 89.68(6) 2_666 . ?
C2 C1 C4 111.2(4) . . ?
C2 C1 C3 111.6(4) . . ?
C4 C1 C3 110.2(4) . . ?
C2 C1 S1 105.6(3) . . ?
C4 C1 S1 112.7(3) . . ?
C3 C1 S1 105.2(3) . . ?
C6 C5 C8 111.2(5) . . ?
C6 C5 C7 109.8(4) . . ?
C8 C5 C7 109.7(5) . . ?
C6 C5 S2 109.6(4) . . ?
C8 C5 S2 111.6(4) . . ?
C7 C5 S2 104.7(4) . . ?
C11 C9 C12 111.0(13) . . ?
C11 C9 C10 109.4(14) . . ?
C12 C9 C10 109.0(14) . . ?
C11 C9 S3 110.3(11) . . ?
C12 C9 S3 111.0(11) . . ?
C10 C9 S3 105.9(11) . . ?
C12' C9' C10' 112.6(17) . . ?
C12' C9' C11' 110.4(13) . . ?
C10' C9' C11' 108.7(13) . . ?
C12' C9' S3 112.5(12) . . ?
C10' C9' S3 103.2(11) . . ?
C11' C9' S3 109.0(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.888(4) . ?
S1 Al 2.3434(18) 2_666 ?
S1 Al 2.3507(18) . ?
S2 C5 1.862(5) . ?
S2 Al 2.2096(18) . ?
S3 C9 1.84(2) . ?
S3 C9' 1.88(2) . ?
S3 Al 2.2085(18) . ?
Al S1 2.3434(18) 2_666 ?
C1 C2 1.514(7) . ?
C1 C4 1.523(7) . ?
C1 C3 1.530(7) . ?
C5 C6 1.508(8) . ?
C5 C8 1.519(7) . ?
C5 C7 1.530(7) . ?
C9 C11 1.522(9) . ?
C9 C12 1.525(9) . ?
C9 C10 1.531(9) . ?
C9' C12' 1.522(9) . ?
C9' C10' 1.528(9) . ?
C9' C11' 1.530(10) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 S3 Al S2 -49.9(4) . . . . ?
C9' S3 Al S2 -62.9(4) . . . . ?
C9 S3 Al S1 176.9(4) . . . 2_666 ?
C9' S3 Al S1 163.9(4) . . . 2_666 ?
C9 S3 Al S1 80.7(4) . . . . ?
C9' S3 Al S1 67.7(4) . . . . ?
C5 S2 Al S3 -64.1(2) . . . . ?
C5 S2 Al S1 66.68(19) . . . 2_666 ?
C5 S2 Al S1 164.00(18) . . . . ?
C1 S1 Al S3 -128.67(18) . . . . ?
Al S1 Al S3 107.75(8) 2_666 . . . ?
C1 S1 Al S2 9.81(19) . . . . ?
Al S1 Al S2 -113.77(8) 2_666 . . . ?
C1 S1 Al S1 123.58(19) . . . 2_666 ?
Al S1 Al S1 0.0 2_666 . . 2_666 ?
Al S1 C1 C2 178.8(3) 2_666 . . . ?
Al S1 C1 C2 70.3(4) . . . . ?
Al S1 C1 C4 57.2(4) 2_666 . . . ?
Al S1 C1 C4 -51.4(4) . . . . ?
Al S1 C1 C3 -63.0(4) 2_666 . . . ?
Al S1 C1 C3 -171.6(3) . . . . ?
Al S2 C5 C6 -73.8(4) . . . . ?
Al S2 C5 C8 49.9(5) . . . . ?
Al S2 C5 C7 168.5(3) . . . . ?
C9' S3 C9 C11 177(4) . . . . ?
Al S3 C9 C11 99.3(9) . . . . ?
C9' S3 C9 C12 54(3) . . . . ?
Al S3 C9 C12 -24.1(11) . . . . ?
C9' S3 C9 C10 -65(4) . . . . ?
Al S3 C9 C10 -142.4(8) . . . . ?
C9 S3 C9' C12' -56(3) . . . . ?
Al S3 C9' C12' 50.4(12) . . . . ?
C9 S3 C9' C10' 65(4) . . . . ?
Al S3 C9' C10' 172.1(9) . . . . ?
C9 S3 C9' C11' -179(4) . . . . ?
Al S3 C9' C11' -72.4(9) . . . . ?
